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A kind of method for preparing bis(norbornadiene) tetrafluoroborate rhodium

A technology of rhodium tetrafluoroborate and norbornanol, which is applied in chemical instruments and methods, purification/separation of hydrocarbons, organic chemistry, etc., can solve the problems of high preparation cost, cumbersome process, low yield, etc., and achieve improved yield and Purity, simple preparation method, and the effect of reducing production costs

Active Publication Date: 2022-08-02
XIAN CATALYST NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Bis(norbornadiene) rhodium tetrafluoroborate has unstable physical and chemical properties and is prone to react with oxygen. The existing preparation method has complex processes, low yield and high preparation cost, which is unfavorable for popularization and use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A method for preparing bis(norbornadiene) rhodium tetrafluoroborate, comprising the following steps:

[0024] (1) Take rhodium trichloride hydrate and norbornadiene in a ratio of 1:3.0 according to the amount of substances, put them in methanol solvent that has been deoxygenated in advance, and heat to reflux, the reflux temperature is 75 ℃, and the reflux time for 3h, then concentrated and filtered to obtain norbornadiene rhodium chloride dimer;

[0025] (2) under the environment of nitrogen protection, the norbornadiene rhodium chloride dimer obtained in step (1) is dissolved in the dichloromethane solvent that has undergone pre-deoxidation treatment, and then silver tetrafluoroborate is added to carry out ion exchange reaction , the reaction time is 10h, obtains bis(norbornadiene) tetrafluoroborate rhodium solution;

[0026] Wherein, the ratio of the amount of norbornadiene rhodium chloride dimer to silver tetrafluoroborate is 1:2.5;

[0027] (3) Under the environm...

Embodiment 2

[0029] A method for preparing bis(norbornadiene) rhodium tetrafluoroborate, comprising the following steps:

[0030] (1) Take rhodium trichloride hydrate and norbornadiene in a ratio of 1:6.0 according to the amount of substances, place them in an ethanol solvent that has been deoxygenated in advance, and heat under reflux at a reflux temperature of 85°C and a reflux time. for 1h, then concentrated and filtered to obtain norbornadiene rhodium chloride dimer;

[0031] (2) Under the environment of argon protection, the norbornadiene rhodium chloride dimer obtained in step (1) is dissolved in the 1,2-dichloroethane solvent that has undergone pre-deoxidation treatment, and then tetrafluoroboric acid is added. Silver, carry out ion exchange reaction, and the reaction time is 18h to obtain bis(norbornadiene) tetrafluoroborate rhodium solution;

[0032] Wherein, the ratio of the amount of norbornadiene rhodium chloride dimer to silver tetrafluoroborate is 1:3.0;

[0033] (3) Under ...

Embodiment 3

[0035] A method for preparing bis(norbornadiene) rhodium tetrafluoroborate, comprising the following steps:

[0036] (1) Take rhodium trichloride hydrate and norbornadiene in a ratio of 1:5.0 according to the amount of matter, place them in an ethanol solvent that has been deoxygenated in advance, and heat to reflux at a reflux temperature of 80°C and a reflux time of 80°C. for 2h, then concentrated and filtered to obtain norbornadiene rhodium chloride dimer;

[0037] (2) under the environment of argon protection, the norbornadiene rhodium chloride dimer obtained in step (1) is dissolved in the chloroform solvent that has undergone pre-deoxidation treatment, and then silver tetrafluoroborate is added to carry out ion exchange reaction, The reaction times was 15h, and bis(norbornadiene) rhodium tetrafluoroborate solution was obtained;

[0038] Wherein, the ratio of the amount of norbornadiene rhodium chloride dimer to silver tetrafluoroborate is 1:3.5;

[0039] (3) Under the ...

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Abstract

The invention belongs to the technical field of precious metal preparation, and relates to a method for preparing bis(norbornadiene) rhodium tetrafluoroborate. After ion exchange reaction with silver tetrafluoroborate, red bis(norbornadiene) rhodium tetrafluoroborate solid is obtained by pressure filtration. The preparation method is simple, and the yield and purity of bis(norbornadiene) rhodium tetrafluoroborate product are improved. , reducing production costs.

Description

technical field [0001] The invention belongs to the technical field of precious metal preparation, relates to the synthesis of a rhodium complex, in particular to a method for preparing bis(norbornadiene) rhodium tetrafluoroborate. Background technique [0002] Metal rhodium complexes are widely used in metal-organic chemistry and organic synthetic chemistry. Rhodium bis(norbornadiene)tetrafluoroborate is not only a raw material for the synthesis of many complex metal rhodium complexes, but also often used together with other ligands to jointly catalyze the occurrence of many reactions such as coupling, hydrogenation and addition. [0003] The rhodium bis(norbornadiene)tetrafluoroborate has unstable physical and chemical properties, and is easy to react with oxygen. The existing preparation method is complicated in process, low in yield, and high in preparation cost, which is unfavorable for popularization and use. SUMMARY OF THE INVENTION [0004] In view of the above pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C2/38C07C7/00C07C13/42
CPCC07C2/38C07C7/005C07C2602/42C07C13/42
Inventor 张高鹏潘丽娟朱大川韩彬
Owner XIAN CATALYST NEW MATERIALS CO LTD
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